JP3492043B2 - Surface treatment method for resin pellets - Google Patents

Description

Description: BACKGROUND OF THE INVENTION 1. Field of the Invention
The present invention relates to a surface treatment method for imparting moldability. [0002] Generally, adhesives, adhesives, rubbers, and elastomers
Pellet resin with self-adhesive or adhesive properties, such as
If the pellets are used, the pellets
Causes blocking and becomes a large lump, handling work
However, there is a problem that the performance is significantly reduced. [0003] Various attempts have been made to address the above problems.
For example, in Japanese Patent Publication No. 7-37026,
Extrudes the adhesive resin from the extruder and pellets in water
And resin pellet surface, silica powder, clay,
Talc, mica, quartz sand, shirasu, magnesium carbonate, carbonic acid
Inorganic powder such as calcium, polyethylene wax, E
Coated with anti-adhesion powder such as organic powder such as VA
After that, dry while circulating the resin pellets
A method for producing a characteristic resin pellet has been proposed. However, among the above proposals, inorganic powders
When used as an anti-adhesion powder, blocking can be prevented.
However, when resin pellets are made into a solution, inorganic powder
There is a problem of separation and sedimentation.
When the melt is hot melted, the inorganic powder
There is a problem of clogging the menu. [0005] Among the above proposals, organic powders are used to prevent sticking.
When used as a stopping powder, the organic powder is
Dissolution or melting by heating.
Does not cause clogging, but has an anti-blocking effect
Poorer than inorganic powder or obtained from resin pellets
For example, the performance of the final product such as an adhesive
There are problems such as lowering. Further, stearin is used as an anti-adhesion powder.
Metal soap powders such as zinc oxide and ethylenebisamide
Fatty acid amide-based powders are also used,
Since these also belong to organic powders, the same problems as above
There is. SUMMARY OF THE INVENTION The present invention relates to the conventional
Excellent blocking resistance to solve problems
In addition, when final products such as adhesives are used,
No separation, sedimentation, clogging, etc.
Does not degrade the final performance of the product, such as adhesive strength
Surface treatment of resin pellets from which resin pellets can be obtained
It is an object to provide a management method. [0008] A resin pellet according to the present invention.
Surface treatment method, the degree of polymerization is 300-5000
Containing at least 50 mol% of vinyl alcohol units
Saponified polyvinyl acetate (co) polymer (hereinafter referred to as
With respect to 1 equivalent of a hydroxyl group of “(a) component”),
Cyanate group, carboxylic acid group, acid halide group, ketene
Group selected from the group consisting of
Functional groups capable of reacting with one or more hydroxyl groups
A long-chain alkyl having 6 to 30 carbon atoms in the alkyl group
(Hereinafter referred to as "component (b)") in terms of functional group
The release agent component obtained by reacting at least 0.5 equivalents with
Fatty acids having a prime number of 10 to 30 or metal salts thereof (hereinafter referred to as
Below, it is described as “(c) component”) and / or an acid value of 0.1.
2-800 acid-modified polyolefin (co) polymer
(Hereinafter referred to as “component (d)”) and dispersed in water.
A water-dispersed release agent composition consisting of
After that, it is characterized by drying.
Is achieved. [0009] A method for surface treatment of resin pellets according to the present invention.
(A) constituting the aqueous dispersion release agent composition used for
Saponified polyvinyl acetate (co) polymer as
Consistency 300-5000, preferably 800-250
0, and the vinyl alcohol unit is 50 mol% or less.
Above, preferably at least 60 mol%.
It is important. Incidentally, the polyvinyl acetate (co) polymer mentioned here
Is the saponification of a homopolymer of vinyl acetate monomer.
Product, or vinyl acetate monomer and the vinyl acetate monomer
A saponified copolymer of a copolymerizable polymerizable monomer with
means. A saponified product of the above-mentioned polyvinyl acetate copolymer
Although not particularly limited, ethylene and
Between vinyl monomers such as lylic acid and vinyl acetate monomers
Saponified copolymer, specifically, ethylene-vinyl acetate
Saponified copolymer, acrylic acid-vinyl acetate copolymer
Saponified products and the like, and one or more of these are
It is preferably used. A saponified product of the above polyvinyl acetate (co) polymer
Is less than 300, the resulting release agent component
The releasability becomes insufficient and the polymerization degree exceeds 5,000
Then, the obtained release agent component becomes difficult to disperse in water. The above-mentioned polyvinyl acetate (co) polymer soap
Content of vinyl alcohol unit in the compound is 50 mol%
If it is less than 1, the content of the hydroxyl group becomes small,
(B) Reactivity with component (b) is reduced, resulting in a release agent component
The mold release property becomes poor. The vinyl alcohol used here
Is the content of polyvinyl acetate (co) polymer
Based on the total number of units of the monomers constituting the saponified product
Of the number of units of the converted vinyl acetate monomer (mol
%). [0013] Surface treatment method for resin pellets according to the present invention
(B) constituting the aqueous dispersion release agent composition used for
Long-chain alkyl compound as an isocyanate group,
Carboxylic acid group, acid halide group, ketene group, aldehyde group
One or two selected from the group consisting of
Having a functional group capable of reacting with at least one kind of hydroxyl group,
When the carbon number of the alkyl group is 6 to 30, preferably 8 to 28,
It is necessary to be. The carbon of the alkyl group of the long-chain alkyl compound
When the prime number is less than 6, the release property of the obtained release agent component is
Insufficient, conversely, the alkyl group has more than 30 carbon atoms
And a polyvinyl acetate (co) polymer soap as the component (a)
Reactivity with the compound is reduced. As a functional group capable of reacting with a hydroxyl group, isocyanate
It has a nate group, and the carbon number of the alkyl group is 6 to 30.
The long-chain alkyl compound is not particularly limited.
Not available, but hexyl isocyanate, octyl isocyanate
Salt, dodecyl isocyanate, octadecyl isocyanate
And docosanyl isocyanate.
One or more of these are suitably used. Carboxyl is a functional group capable of reacting with a hydroxyl group.
A long chain having an acid group and an alkyl group having 6 to 30 carbon atoms
The alkyl compound is not particularly limited.
But octanoic acid, dodecanoic acid, octadecanoic acid, docosa
And one or more of these are preferred.
Appropriately used. As a functional group capable of reacting with a hydroxyl group, acid
Chain having an alkyl group having 6 to 30 carbon atoms
The alkyl compound is not particularly limited.
But octanoyl chloride, dodecanoyl chloride
Octadecanoyl chloride, octadecyloylc
Loride, docosanoyl chloride, etc.
One or more of these are suitably used. In addition, ketones as functional groups capable of reacting with hydroxyl groups
Chain having an alkyl group and 6 to 30 carbon atoms in the alkyl group
The alkyl compound is not particularly limited.
But octyl ketene dimer, dodecyl ketene dimer
ー, octadecyl ketene dimer, docosanil ketenda
And one or more of these.
It is preferably used. Further, as a functional group capable of reacting with a hydroxyl group,
It has an aldehyde group and the alkyl group has 6 to 30 carbon atoms.
Certain long-chain alkyl compounds are particularly limited
Not hexylaldehyde, octylaldehyde
Do, dodecylaldehyde, octadecylaldehyde, do
Cosanilaldehyde and the like; one or more of these
Two or more are preferably used. Further, a functional group capable of reacting with a hydroxyl group is used.
Having an epoxy group, wherein the alkyl group has 6 to 30 carbon atoms.
Certain long-chain alkyl compounds are particularly limited
Not octyl glycidyl ether, dodecyl
Lysidyl ether, octadecyl glycidyl ether,
Docosanyl glycidyl ether; and the like.
One or more kinds are suitably used. [0021] Surface treatment method for resin pellets according to the present invention
Release agent component in aqueous dispersion release agent composition used for
Is a polyvinyl acetate (co) polymer as the component (a)
Component (b) with respect to 1 equivalent of the hydroxyl group of the saponified product of
Long chain alkyl compound is 0.5 equivalent or more in terms of functional group,
Preferably, at least 0.6 equivalent is reacted.
is necessary. (A) Poly (vinyl acetate)
It is the component (b) with respect to one equivalent of the hydroxyl group of the combined saponified product.
The ratio of long-chain alkyl compounds is less than 0.5 equivalent in terms of functional groups.
If it is full, the release properties of the obtained release agent component will be insufficient.
You. The method of synthesizing the release agent component is a special one.
Instead, in a solvent, polyvinyl acetate as component (a)
(B) relative to 1 equivalent of the hydroxyl group of the saponified (co) polymer
The long-chain alkyl compound is 0.5 equivalent
By reacting at a ratio such that the
Release agent component can be obtained. The solvent used in the synthesis of the release agent component
The type is not particularly limited, but the component (b)
Depending on the type of functional group of a long-chain alkyl compound
It is preferable that it is appropriately selected. That is, the long-chain alkyl compound as the component (b)
The functional group of the product is an isocyanate group or a ketene group
, Such as toluene and dimethyl sulfoxide
Inactive which does not react with various isocyanate groups or ketene groups
Performing the reaction by a suspension method or dissolution method using a neutral solvent
Is preferred. The component (b) contains a long-chain alkyl compound.
When the functional group to be reacted is a carboxylic acid group, such as toluene
Reaction using the solvent used for normal esterification
Is preferably performed. Also, a long-chain alkyl compound as the component (b)
When the functional group of is an acid halide group, the acid halide
The reaction can be carried out using an inert solvent that does not react with the group.
Preferably, during this reaction, a dehalogenation such as pyridine is performed.
More preferably, a hydrogenation agent is added. Further, the long-chain alkylation as the component (b)
When the functional group of the compound is an aldehyde group,
Perform the reaction using an inert solvent that does not react with the
However, during this reaction, an acid catalyst such as hydrochloric acid is used.
Is more preferably added. Furthermore, a long-chain alkyl which is the component (b)
When the functional group of the compound is an epoxy group,
Performing the reaction using an inert solvent that does not react with the group
However, during this reaction, sodium hydroxide is preferably used.
It is more preferable to add such an alkali catalyst. Reaction between component (a) and component (b) described above
Is the length of the component (b) according to the infrared absorption spectrum and the like.
Of a functional group that can react with the hydroxyl group of the
It is terminated when the disappearance is confirmed in effect. The surface treatment method for resin pellets according to the present invention
In the aqueous dispersion release agent composition used for (c), (c)
Fatty acids having 10 to 30 carbon atoms or
Are used. The above fatty acids or metal salts thereof
Is obtained by reacting the components (a) and (b).
The above-mentioned release agent component is emulsified and dispersed uniformly and stably in water.
Function. Constituting the above aqueous dispersion release agent composition
The fatty acid or its metal salt as the component (c) is a carbon
The number is 10-30, preferably 12-26
is necessary. The carbon number of the above fatty acid or its metal salt is
If it is less than 10, the polarity becomes too high and the release agent component
Separation or separation of the aqueous dispersion resulting from the melting point being too low
It reduces the releasability of the mold composition. Conversely, if the carbon number is 30
If it exceeds, the polarity becomes too low to be easily dispersed in water. The above fatty acid having 10 to 30 carbon atoms is
Although not particularly limited, for example, dodeca
Acid (lauric acid), hexadecanoic acid (palmitin)
Acid), octadecanoic acid (stearic acid), octadecene
Acid (oleic acid), icosanoic acid (arachidic acid), doco
Saturated or unsaturated fatty acids such as sanic acid (behenic acid)
One or more of these are preferably used
Can be The above fatty acid having 10 to 30 carbon atoms
As the metal salt of the above-mentioned saturated or unsaturated fatty acids,
Alkaline metal water such as sodium hydroxide and barium hydroxide
Oxide or alkaline earth metal hydroxide
Metal salts and the like obtained by
Two or more are suitably used. The component (c) in the aqueous dispersion release agent composition
Content is not particularly limited, but (a)
The aforementioned release agent obtained by reacting the component and the component (b).
Component (c) is 1 to 50 parts by weight based on 100 parts by weight of the component.
And preferably 3 to 40 parts by weight.
Is more preferable. (C) Component based on 100 parts by weight of release agent component
If the content is less than 1 part by weight, the aqueous dispersion release agent set
Uniform and stable release agent components in water when producing products
It becomes difficult to emulsify and disperse in
The content of the component (c) is 50 parts by weight with respect to 00 parts by weight.
If it exceeds, it can be manufactured using surface-treated resin pellets.
The final product such as adhesive strength
Performance decreases. Surface treatment method for resin pellets according to the present invention
In the aqueous dispersion release agent composition used for (a), (d)
Acid-modified polyole having an acid value of 0.2 to 800 as a component
Fin (co) polymers are used. The above acid-modified polyole
The fin (co) polymer is, like the component (c) described above,
The above-mentioned component obtained by reacting the component (a) with the component (b)
A machine for uniformly and stably emulsifying and dispersing release agent components in water
Has ability. The acid-modified polyolefin mentioned here
(Co) polymer is an acid-modified polyolefin alone
Polymer or copolymer of acid-modified polyolefin
Means Constituting the aqueous dispersion release agent composition
Acid-modified polyolefin (co) polymer as component (d)
Has an acid value of 0.2 to 800, preferably 10 to 200,
It is necessary to be. The above acid-modified polyolefin (co) polymer
When the acid value is less than 0.2, the dispersion in water itself is
On the contrary, if the acid value exceeds 800, the release agent component
Easy and stable, uniform and stable aqueous dispersion release agent
It is difficult to obtain a product. The component (d) is particularly limited.
Although not intended, ethylene, propylene, 1-butene, etc.
Olefin and acrylic acid, methacrylic acid, maleic
Has polar groups such as acid, itaconic acid and vinylpyrrolidone
Copolymers with vinyl monomers, chemically or physically
Oxidized polyethylene, polypropylene, polybu
And polyolefin (co) polymers such as
One or more of these are suitably used. The above-mentioned olefin and a vinyl group having a polar group
Specific examples of the copolymer with the monomer are not particularly limited.
Although not necessarily, for example, ethylene-acrylic acid copolymer
Merged or maleic acid-modified or acrylic acid-modified polye
Tylene wax and the like.
More than one species is preferably used. Further, the olefin and a vinyl having a polar group
Occupy in the copolymer in the case of a copolymer with
The content of the vinyl monomer having a polar group is particularly limited.
It is not limited to 0.01 to 40 mol%
And preferably 0.5 to 10 mol%.
Is more preferred. The polymerization degree of the component (d) is not particularly limited.
Although it is not a thing, it is preferably 10 to 2000
In particular, it is more preferable to be 20 to 1000
No. If the degree of polymerization of component (d) is less than 10,
Since it is in a softened state even at room temperature, the resulting aqueous dispersion
The release property of the release agent composition deteriorates, and conversely, the polymerization degree becomes 2000
When it exceeds, it becomes difficult to disperse itself in water. The melting point and melt viscosity of the component (d)
Is not particularly limited, but has a melting point of 40 ° C. or higher.
And the melt viscosity at 140 ° C. is 10,000 (Pa ·
s) It is preferably at most, especially having a melting point of 60 ° C.
As described above, the melt viscosity at 140 ° C. is 5000 (Pa ·
s) More preferably, When the melting point of component (d) is less than 40 ° C.,
The release property of the obtained aqueous dispersion release agent composition becomes insufficient.
And the melt viscosity at 140 ° C. is 10,000 (Pa)
If it exceeds s), it will be difficult to disperse itself in water. Further, in the aqueous dispersion type release agent composition,
The content of the component (d) is not particularly limited.
Is obtained by reacting the component (a) with the component (b).
1 to 50 parts by weight with respect to 100 parts by weight of the aforementioned release agent component
Preferably, the amount is 3 to 40 parts by weight.
Is more preferable. (D) Component based on 100 parts by weight of release agent component
If the content is less than 1 part by weight, the aqueous dispersion release agent set
Uniform and stable release agent components in water when producing products
It becomes difficult to emulsify and disperse in
The content of the component (d) is 50 parts by weight with respect to 00 parts by weight.
If it exceeds, the release property of the obtained aqueous dispersion release agent composition is low.
Down. The surface treatment method for resin pellets according to the present invention
In the aqueous dispersion release agent composition used for the
The component (c) and the component (d) are each used alone.
Or both components may be used in combination. When component (c) and component (d) are used in combination,
Although the content is not particularly limited, the component (a)
The above-mentioned release agent component obtained by reacting component (b)
The sum of the components (c) and (d) with respect to 100 parts by weight
The amount is preferably 1 to 50 parts by weight, and especially 3 to 50 parts by weight.
More preferably, it is 40 parts by weight. The reason is,
When component (c) or component (d) is used alone
Is the same as The surface treatment method for resin pellets according to the present invention
The aqueous dispersion release agent composition used for
(B) the aforementioned release agent component obtained by reacting the component with the component,
In addition to the component (c) and / or the component (d),
Release agent components as needed as long as they do not interfere with the purpose of
Of water dispersion in water
The wettability and film forming property when the agent composition adheres to the resin surface.
High boiling liquid substances to improve or suppress foaming
The strength of the dried film of the surfactant and the aqueous dispersion release agent composition
One or two kinds of various additives such as a cross-linking agent for raising
The above may be contained. The high-boiling liquid substance is not particularly limited.
But the boiling point under normal pressure is 100 ° C or higher,
Those whose viscosity at room temperature is 1000 (Pa · s) or less
preferable. It is also manufactured using surface-treated resin pellets.
Must not interfere with the performance of the final product
preferable. The boiling point of the above high boiling point liquid substance under normal pressure is 1
When the temperature is lower than 00 ° C., the obtained aqueous dispersion release agent composition
It is easy to volatilize when coating and drying.
Required, leading to increased manufacturing costs. Also, the above high
The viscosity at room temperature of the boiling liquid substance is 1000 (Pa · s)
If it exceeds, the fluidity becomes low, so the aqueous dispersion release agent composition
The effect of improving the wettability and film forming property of the object becomes poor. The high boiling point liquid substance is not particularly limited.
Although not limited to, for example, naphthenic oils,
Phosphorus, oligomers of olefins, vegetable oils, animal oils, minerals
Process oil such as material oil, liquid rosin, turpentine oil, etc.
Liquid tackifier resin, polybutene, diisodecyl phthalate
And one or two of these.
The above is preferably used. As the surfactant, nonionic surfactants can be used.
Surfactants, anionic surfactants, cationic surfactants
Any of amphoteric agents and amphoteric surfactants can be used,
One or more of these are suitably used. Further, as the crosslinking agent, an aqueous dispersion
During film formation after attaching the mold composition to the resin surface, heat,
Any material that can be crosslinked by reacting with the release agent component by light or the like is acceptable.
Is not particularly limited, for example, polyvalent iso
Cyanate compound, blocked polyvalent isocyanate compound
Substances, polyepoxy compounds, polyacryloyl compounds,
Polymethylol compound, polyvalent ionic metal, polyvalent aziridine
And the like. One or more of these compounds
It is preferably used. For surface treatment of resin pellets according to the present invention
In the aqueous dispersion release agent composition to be used, the component (a)
The above-mentioned release agent component obtained by reacting component (b)
Together with the component (c) and / or the component (d),
One of various additives such as point liquid substance, surfactant, cross-linking agent
Or, when two or more kinds are contained as necessary,
Including these, it is necessary to be dispersed in water
You. The method for producing the aqueous dispersion release agent composition is as follows.
Although not particularly limited, for example, (a)
A release agent component obtained by reacting the component with the component (b);
(C) component and / or (d) component, and, if necessary,
Consists of one or more of various additives to be contained
The release agent composition is heated and melted in advance, and the heated melt is mixed with water.
The pressure kneader, colloid mill, high speed stirring
Using a mixer such as a soft mixer, apply high shear to uniformly emulsify
After dispersing, cool so that the dispersed particles do not fuse and aggregate
Method for Obtaining Desired Water-Dispersed Release Agent Composition (High-Pressure Emulsification Method)
Alternatively, the release agent composition is dissolved in an organic solvent in advance, and the
Apply high shear to the liquid and water using, for example, a high-speed emulsifier.
After uniformly emulsifying and dispersing, remove the organic solvent and remove
A method of obtaining a water-dispersed release agent composition (solvent dissolution method) and the like are listed.
Both methods are suitably adopted, but among them,
High pressure emulsification method that does not require removal of organic solvent and has simple process
It is preferably adopted. In the above high-pressure emulsification method, the release agent composition
The heating and melting temperature is not particularly limited.
0 ° C. or higher, and the temperature of water is particularly
Although it is not limited, the temperature is increased to 100 ° C. or more by pressurization.
It is preferred that In the high-pressure emulsification method, a release agent
Put the product into water at once without heating and melting the product
And apply high shear at a temperature of about 120 ° C under pressure
After emulsifying and dispersing, the desired aqueous dispersion release agent set is cooled.
A method for obtaining a product may be employed. Any of the above high pressure emulsification method or solvent dissolution method
Also in these methods, the mixing ratio of the release agent composition and water
Is not particularly limited, the release agent composition 5
Preferably 50% by weight and 95-50% by weight of water
No. If the content of the release agent composition is less than 5% by weight, milk
The shearing effect at the time of dispersing is reduced, reducing the production efficiency,
If the content of the release agent composition exceeds 50% by weight,
Becomes too high, making uniform emulsification and dispersion difficult. The water obtained through the above emulsification and dispersion step
The dispersing release agent composition should be used within a range that does not impair the storage stability.
If necessary, it may be diluted with water. The surface treatment of resin pellets according to the present invention
The resin that can be an elephant is not particularly limited.
However, self-adhesion of adhesives, adhesives, rubber, elastomers, etc.
And those having adhesive properties.
Rubber, isoprene rubber, butyl rubber, isobutylene rubber,
Styrene butadiene rubber, chloroprene rubber, acrylo
Natural or synthetic materials such as nitrile butadiene rubber and chlorinated rubber
Rubber, styrene-butadiene-styrene block copolymer
United, styrene-isoprene-styrene block copolymer
Body, styrene-ethylene-butylene-styrene block
Copolymer, styrene-ethylene-propylene-styrene
Styrenic thermoplastic elastomers such as block copolymers
-, Vinyl chloride-vinyl acetate copolymer, ethylene-acetic acid
Thermoplastic resins such as vinyl copolymers and their adhesive
Made by mixing additives such as imparting resin, softener and filler
Pressure-sensitive adhesives and adhesives, etc., all of which are suitably used.
You. Surface of resin that can be subjected to the above surface treatment
The method of attaching the aqueous dispersion release agent composition described above to
Not special, for example, a water-dispersed release agent composition
After immersing the resin in a filled container, dry it.
May be used, or the aqueous dispersion release agent composition may be applied to the resin surface.
For example, after applying it to the surface by spraying, etc., and then drying it
A law may be adopted. When the surface treatment is performed, the shape of the resin is as follows.
Although not particularly limited, the resin is pelletized in advance.
Surface treatment may be performed in a state where
After performing surface treatment on de-shaped resin, for example, pelletizer
It may be formed into pellets by the method described above. The state of the resin when the above surface treatment is performed
Is not particularly limited, but may be in the form of pellets or
May be in the form of a strand solid,
It can be in the molten state of a rod or strand
In the latter case, the aqueous dispersion release agent composition is used as a cooling agent.
Also works. Further, drying of the surface-treated resin
Is not particularly limited, but forced drying under heating
It may be dried, or it may be naturally dried at room temperature.
Is also good. (Function) Surface of resin pellet according to the present invention
The treatment method is the saponification of a specific polyvinyl acetate (co) polymer.
Reacts with a specific long-chain alkyl compound at a specific ratio.
The release agent component obtained by
Metal salt and / or specific acid-modified polyolefin
Water-dispersed mold release dispersed in water with (co) polymer
After the agent composition is applied to the resin surface and dried,
Resin pellets have excellent blocking resistance
And can be stably stored for a long period of time
Workability at the time is also good. Also, final products such as adhesives
Separation, sedimentation, clogging, etc.
Without reducing the final performance of the final product, such as adhesive strength
Never even. BEST MODE FOR CARRYING OUT THE INVENTION The present invention will be described in more detail.
Examples will be described below. The “parts” in the examples are
It means "parts by weight". (Embodiment 1) 1) Preparation of aqueous dispersion release agent composition Reaction vessel equipped with stirrer, cooler, dropping funnel and thermometer
After charging 50 g of dehydrated xylene, polyacetic acid
Polyvinyl alcohol as a saponified vinyl (co) polymer
(Polymerization degree 1100, containing vinyl alcohol unit
(Amount of 98 mol%) and uniformly dispersed. Next
At reflux temperature, as octadecyl
67 g of isocyanate (1.0 equivalent in terms of functional group),
And dibutyltin dilaurate 0.01 as a polymerization catalyst
g was added and reacted with the above polyvinyl alcohol. Anti
Reaction progresses, and the polyvinyl alcohol powder disappears completely
After that, the reaction was continued for another 2 hours. After the reaction, 4
After cooling to 0 ° C, the reaction solution was dissolved in 1000 g of methanol.
And a white precipitate was obtained. The resulting white precipitate is
After washing with ethanol and then n-hexane, drying
Thus, a release agent component was obtained. 15 parts of the release agent component obtained above, acid-modified
Ethylene-acrylic acid copolymer as polyolefin copolymer
Polymer (acid value 80, polymerization degree 700, acrylic acid content 4
Mol%) 4 parts, alkyl diphenyl ether as a surfactant
-Terdisulfonic acid salt (trade name "Perex SS-
L ", manufactured by Kao Corporation) 0.5 part and polyoxyethylene noni
Luphenyl ether (trade name "Emulgen 910", flower
0.5 part of water and 80 parts of water are mixed, and high-pressure milk is mixed.
Temperature, 120 ℃, stirring speed 500rpm
m for 10 minutes, releasing agent component and ethylene-acrylic acid.
The luic acid copolymer was melted. Next, the temperature was raised to 135 ° C.
Stir at a high speed of 5000 rpm for 1 hour to emulsify and disperse.
After performing, the mixture was cooled to obtain a water-dispersed release agent composition. Next
Then, the obtained water-dispersed release agent composition is diluted with water,
Water-dispersed release agent composition having a release agent composition content of 3% by weight
Object was produced. ( 2) Preparation of resin for pellets Styrene-isoprene-styrene block copolymer (trademark)
Product name "Quintac 3421", manufactured by Zeon Corporation) 10
0 parts, tackifying resin (trade name “ESCOLETS 440”
1 ", manufactured by Tonex Corporation) 100 parts, naphthenic oil
(Product name "Sansen Oil", manufactured by SUNOCO) 50
Parts and an antioxidant (trade name “Yoshinox 42
5 ”, manufactured by Yoshitomi Pharmaceutical Co., Ltd.)
A pressure-sensitive adhesive was prepared. ( 3) Implementation of surface treatment The hot melt adhesive obtained above is made into a strand.
The volume filled with the water-dispersed release agent composition obtained above
After passing through the vessel, pull it up and remove it with a pelletizer.
Let's go. Next, the obtained pellets were further mixed with the above water
After putting into a container filled with the dispersion release agent composition,
Hot, with the release agent composition adhered to the surface
A pellet of the melt adhesive was obtained. ( 4) Evaluation (A) blocking resistance of the pellets obtained above,
(B) stability in solution state, (c) stability in molten state
Properties and (d) performance as an adhesive tape by the following methods
Was evaluated. The results were as shown in Table 1. ( a) Blocking resistance : 7cm diameter, high
Put 20g of pellets in a 10cm glass container,
Thickness 0.5, whose diameter is slightly smaller than the inner diameter of the glass container
mm stainless steel plate, and place 1 mm on the stainless steel plate.
2 weeks in a 40 ° C oven with a weight of 00g
After leaving it for a while, take it out, turn the glass container upside down,
Observe the drop condition of the reticle visually, and
The rocking properties were evaluated. [Judgment criteria] ○ ‥‥ The pellets are broken down one by one and all fall. △ ‥‥ The pellets did not fall, but collapsed when plucked with a stick.
And fell. Further rubbing by hand separated the grains one by one. × ‥‥ Pellets do not fall and fall without breaking even if they are poked with a stick
Did not. However, the outline of the pellet remained. ( b) Stability in solution state : Pellets
Dissolved in Ruen and the pellet content was 30% by weight.
An ene solution was prepared. The solution is then placed in a glass container
After leaving for 2 weeks in an atmosphere of 23 ° C.,
Observe the appearance by visual observation and determine the stability in the solution state according to the following criteria.
Was evaluated. [Judgment criteria] ○ ‥‥ Transparent, no separation or sedimentation was observed. △ ‥‥ Transparent, but separation or sedimentation was observed. × ‥‥ Opaque, and separation or sedimentation was also observed. [0079] c) Stability in the molten state :Hotmelt
Using a coater, apply the pellets to a coating thickness of 12 μm.
To make kraft adhesive tape
Made. At this time, the stainless steel installed in front of the coater
Visually check for clogging of the less mesh filter
Then, stability in a molten state was evaluated according to the following criteria. [Evaluation Criteria] ○ 詰 No clogging was observed × ‥‥ Clogging was observed d) Performance as adhesive tape : JIS
Conforms to Z-0237 "Testing methods for adhesive tapes and sheets"
SP adhesiveness of the kraft adhesive tape obtained above
(G / 15 mm) was measured. Example 2 The composition of the aqueous dispersion release agent composition was
16 parts of the release agent component obtained in Example 1 and stear as fatty acid
3 parts of phosphoric acid (18 carbon atoms)
Kuss SS-L ”0.5 part and“ Emulgen 910 ”0.5 part.
Same as Example 1 except that 5 parts and 80 parts of water were used.
And the aqueous dispersion having a release agent composition content of 3% by weight.
A mold composition was prepared. Next, the obtained aqueous dispersion release agent composition was
The release agent composition was applied to the surface in the same manner as in Example 1.
The pellets of the hot-melt pressure-sensitive adhesive were obtained. (Comparative Examples 1 to 3) Calcium carbonate having an average particle size of 1 μm or less
Fine powder (Comparative Example 1), steer having an average particle diameter of 1 μm or less
Zinc phosphate fine powder (Comparative Example 2), average particle size of 1 μm or less
The following polyethylene fine powder (Comparative Example 3) was
I tried to disperse, but the calcium carbonate fine powder in water
Sedimented, zinc stearate fine powder and polyethylene fine powder
The powder is suspended in water, and a uniform aqueous dispersion is obtained.
Could not. Therefore, in the implementation of the surface treatment,
The surface of the strand-like hot melt adhesive obtained in 1
Then, each of the above three types of fine powder is kept in a fine powder state.
After spraying alone and performing surface treatment, the pelletizer
Hot melt with fine powder adhered to the surface
Thus, three kinds of adhesive pellets were obtained. The results obtained in Example 2 and Comparative Examples 1 to 3 were obtained.
Results of evaluating four types of pellets in the same manner as in Example 1.
Was as shown in Table 1. [Table 1] As shown in Table 1, the surface treatment of the present invention
The resin pellets of Examples 1 and 2 by the method
King properties, stability in solution state, stability in molten state
It is excellent in any case, and can be manufactured using the resin pellet.
The obtained adhesive tape has excellent adhesive strength. On the other hand, as shown in Table 1,
Comparative Example 1 in which surface treatment was performed with fine calcium carbonate powder
Resin pellets have blocking resistance and
Insufficient stability and poor stability in the molten state
No. Also, the ratio of surface treatment with zinc stearate fine powder
The resin pellets of Comparative Example 2 had poor blocking resistance, and
Resin paste of Comparative Example 3 treated with fine ethylene powder
Lett has insufficient blocking resistance and melt
Stability in liquid state and made using the resin pellets
Adhesive tape has poor adhesion. As described above, the surface treatment method of the present invention
According to the method, while having excellent blocking resistance,
Separation, sedimentation, clogging, etc. also occur in the final product
Without degrading the final performance of the final product
Resin pellets without any of them can be easily obtained.

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Claims (1)

(57) [Claims 1] The polymerization degree is 300 to 5000, and based on 1 equivalent of hydroxyl group of a saponified polyvinyl acetate (co) polymer containing 50 mol% or more of a vinyl alcohol unit. Isocyanate group, carboxylic acid group, acid halide group,
A long-chain alkyl compound having a functional group capable of reacting with one or two or more hydroxyl groups selected from the group consisting of a ketene group, an aldehyde group and an epoxy group, wherein the alkyl group has 6 to 30 carbon atoms. The release agent component obtained by reacting at least 0.5 equivalent in conversion is a fatty acid having 10 to 30 carbon atoms or a metal salt thereof, and / or an acid value of 0.2 to
A method for surface treating resin pellets, comprising: adhering a water-dispersed release agent composition dispersed in water together with an acid-modified polyolefin (co) polymer of 800 to a resin surface, followed by drying.